#------------------------------------------------------------------------------
#$Date: 2016-03-26 00:09:44 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180063 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/09/7050963.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7050963
loop_
_publ_author_name
'Montserrat Monfort'
'Inmaculada Resino'
'Joan Ribas'
'Xavier Solans'
'Mercé Font-Bardia'
'Helen Stoeckli-Evans'
_publ_section_title
;
 Four new NiII antiferromagnetic complexes with azido bridges
;
_journal_issue                   11
_journal_name_full               'New J. Chem.'
_journal_page_first              1601
_journal_page_last               1606
_journal_paper_doi               10.1039/b205404c
_journal_volume                  26
_journal_year                    2002
_chemical_formula_moiety         trans-[Ni(N-Pren)2(mu1,3-N3)]n(ClO4)n
_chemical_formula_sum            'C10 H28 Cl N7 Ni O4'
_chemical_formula_weight         404.61
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.958(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.3715(7)
_cell_length_b                   18.4000(12)
_cell_length_c                   12.2042(9)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.97
_cell_measurement_theta_min      2.45
_cell_volume                     1869.7(2)
_computing_cell_refinement       'CELL (Stoe & Cie GmbH, Darmstadt, 1996)'
_computing_data_collection       'EXPOSE (Stoe & Cie GmbH, Darmstadt, 1996)'
_computing_data_reduction
'INTEGRATE (Stoe & Cie GmbH, Darmstadt, 1996)'
_computing_molecular_graphics    'Xtal_GX (Hall & du Boulay, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 0.81
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'STOE Image Plate Diffraction system'
_diffrn_measurement_method       'Phi rotation'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0573
_diffrn_reflns_av_sigmaI/netI    0.0626
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14522
_diffrn_reflns_theta_full        25.97
_diffrn_reflns_theta_max         25.97
_diffrn_reflns_theta_min         2.45
_exptl_absorpt_coefficient_mu    1.141
_exptl_absorpt_correction_T_max  0.8944
_exptl_absorpt_correction_T_min  0.6277
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'pale purple-blus'
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.430
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.052
_refine_ls_extinction_coef       0.0013(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.801
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     231
_refine_ls_number_reflns         3628
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.813
_refine_ls_R_factor_all          0.0781
_refine_ls_R_factor_gt           0.0381
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0510P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0821
_refine_ls_wR_factor_ref         0.0915
_reflns_number_gt                1986
_reflns_number_total             3628
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b205404c.txt
_cod_data_source_block           for_Compound1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0510P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0510P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 2(1)/c'
_cod_database_code               7050963
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.14304(5) 0.27188(3) 0.86736(3) 0.05287(16) Uani 1 d . . .
N1 N 0.2478(4) 0.3756(2) 0.9014(3) 0.0807(10) Uani 1 d . . .
H1N1 H 0.3180 0.3691 0.9627 0.121 Uiso 1 calc R . .
N2 N -0.0728(3) 0.3276(2) 0.8761(3) 0.0738(10) Uani 1 d . . .
H2AN H -0.1440 0.3158 0.8185 0.111 Uiso 1 calc R . .
H2BN H -0.1152 0.3161 0.9386 0.111 Uiso 1 calc R . .
N3 N 0.0371(4) 0.16827(18) 0.8368(2) 0.0665(8) Uani 1 d . . .
H3N3 H -0.0365 0.1734 0.7770 0.100 Uiso 1 calc R . .
N4 N 0.3574(3) 0.2152(2) 0.8585(2) 0.0690(9) Uani 1 d . . .
H4AN H 0.3954 0.2233 0.7933 0.103 Uiso 1 calc R . .
H4BN H 0.4318 0.2297 0.9126 0.103 Uiso 1 calc R . .
N5 N 0.1094(5) 0.2945(2) 0.6968(2) 0.0915(12) Uani 1 d . . .
N6 N 0.1436(3) 0.26769(17) 0.61816(19) 0.0528(7) Uani 1 d . . .
N7 N 0.1776(5) 0.2591(2) 1.0409(2) 0.1091(16) Uani 1 d . . .
C1 C 0.1133(7) 0.4204(3) 0.9391(5) 0.123(2) Uani 1 d . . .
H1A H 0.1024 0.4098 1.0158 0.148 Uiso 1 calc R . .
H1B H 0.1385 0.4716 0.9332 0.148 Uiso 1 calc R . .
C2 C -0.0352(6) 0.4050(3) 0.8739(5) 0.1136(18) Uani 1 d . . .
H2A H -0.0278 0.4202 0.7985 0.136 Uiso 1 calc R . .
H2B H -0.1211 0.4325 0.9021 0.136 Uiso 1 calc R . .
C3 C 0.3410(8) 0.4092(5) 0.8219(5) 0.152(3) Uani 1 d D . .
H3A H 0.2670 0.4360 0.7704 0.183 Uiso 0.50 calc PR A 1
H3B H 0.3857 0.3705 0.7806 0.183 Uiso 0.50 calc PR A 1
H3C H 0.2794 0.4021 0.7509 0.183 Uiso 0.50 d PR A 2
H3D H 0.3382 0.4610 0.8365 0.183 Uiso 0.50 d PR A 2
C4A C 0.4719(17) 0.4581(10) 0.8591(16) 0.183(9) Uani 0.564(18) d PD B 1
H4A H 0.5413 0.4370 0.9194 0.220 Uiso 0.564(18) calc PR B 1
H4B H 0.4317 0.5045 0.8824 0.220 Uiso 0.564(18) calc PR B 1
C5A C 0.557(4) 0.466(2) 0.760(3) 0.34(3) Uani 0.564(18) d PD B 1
H5A H 0.5694 0.4194 0.7270 0.505 Uiso 0.564(18) calc PR B 1
H5B H 0.6607 0.4874 0.7796 0.505 Uiso 0.564(18) calc PR B 1
H5C H 0.4957 0.4972 0.7077 0.505 Uiso 0.564(18) calc PR B 1
C4B C 0.4812(14) 0.3933(11) 0.8053(12) 0.106(7) Uani 0.436(18) d PD B 2
H4C H 0.4785 0.3480 0.7645 0.128 Uiso 0.436(18) calc PR B 2
H4D H 0.5423 0.3847 0.8760 0.128 Uiso 0.436(18) calc PR B 2
C5B C 0.571(3) 0.450(2) 0.743(2) 0.23(2) Uani 0.436(18) d PD B 2
H5D H 0.5103 0.4604 0.6737 0.339 Uiso 0.436(18) calc PR B 2
H5E H 0.6743 0.4306 0.7298 0.339 Uiso 0.436(18) calc PR B 2
H5F H 0.5854 0.4933 0.7859 0.339 Uiso 0.436(18) calc PR B 2
C6 C 0.1668(5) 0.1213(2) 0.8017(3) 0.0827(12) Uani 1 d . . .
H6A H 0.1791 0.1299 0.7246 0.099 Uiso 1 calc R . .
H6B H 0.1393 0.0706 0.8105 0.099 Uiso 1 calc R . .
C7 C 0.3213(5) 0.1383(3) 0.8708(4) 0.0875(14) Uani 1 d . . .
H7A H 0.3111 0.1273 0.9474 0.105 Uiso 1 calc R . .
H7B H 0.4076 0.1089 0.8470 0.105 Uiso 1 calc R . .
C8 C -0.0501(5) 0.1374(3) 0.9258(3) 0.0878(14) Uani 1 d . . .
H8A H 0.0289 0.1198 0.9835 0.105 Uiso 1 calc R . .
H8B H -0.1083 0.1766 0.9571 0.105 Uiso 1 calc R . .
C9 C -0.1631(7) 0.0788(3) 0.8964(5) 0.129(2) Uani 1 d . . .
H9A H -0.1056 0.0372 0.8712 0.154 Uiso 1 calc R . .
H9B H -0.2403 0.0945 0.8362 0.154 Uiso 1 calc R . .
C10 C -0.2520(6) 0.0562(4) 0.9940(5) 0.148(3) Uani 1 d . . .
H10A H -0.3172 0.0143 0.9743 0.222 Uiso 1 calc R . .
H10B H -0.3191 0.0955 1.0134 0.222 Uiso 1 calc R . .
H10C H -0.1755 0.0446 1.0556 0.222 Uiso 1 calc R . .
Cl1 Cl 0.65329(10) 0.30700(7) 1.12008(7) 0.0743(3) Uani 1 d . . .
O1 O 0.7900(4) 0.3527(2) 1.1176(3) 0.1155(12) Uani 1 d . . .
O2 O 0.5132(4) 0.3483(2) 1.1259(3) 0.1259(13) Uani 1 d . . .
O3 O 0.6359(4) 0.2679(3) 1.0208(3) 0.1439(17) Uani 1 d . . .
O4 O 0.6742(5) 0.2644(2) 1.2156(3) 0.1313(14) Uani 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0020 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0040 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0080 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1320 0.1590 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.2850 1.1130 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N4 Ni1 N2 179.39(14) . . ?
N4 Ni1 N5 94.28(13) . . ?
N2 Ni1 N5 85.77(13) . . ?
N4 Ni1 N3 83.55(13) . . ?
N2 Ni1 N3 95.84(13) . . ?
N5 Ni1 N3 89.60(14) . . ?
N4 Ni1 N7 88.13(15) . . ?
N2 Ni1 N7 91.87(16) . . ?
N5 Ni1 N7 175.03(17) . . ?
N3 Ni1 N7 95.00(13) . . ?
N4 Ni1 N1 96.87(14) . . ?
N2 Ni1 N1 83.73(14) . . ?
N5 Ni1 N1 91.48(15) . . ?
N3 Ni1 N1 178.81(12) . . ?
N7 Ni1 N1 83.91(14) . . ?
C3 N1 C1 116.4(5) . . ?
C3 N1 Ni1 119.6(4) . . ?
C1 N1 Ni1 104.2(3) . . ?
C2 N2 Ni1 106.8(3) . . ?
C8 N3 C6 114.7(3) . . ?
C8 N3 Ni1 116.4(3) . . ?
C6 N3 Ni1 105.6(2) . . ?
C7 N4 Ni1 106.9(2) . . ?
N6 N5 Ni1 136.4(3) . . ?
N7 N6 N5 179.6(4) 4_565 . ?
N6 N7 Ni1 149.8(3) 4_566 . ?
C2 C1 N1 110.8(4) . . ?
C1 C2 N2 111.0(5) . . ?
C4B C3 N1 126.3(8) . . ?
C4B C3 C4A 60.3(8) . . ?
N1 C3 C4A 119.8(8) . . ?
C3 C4A C5A 102.6(19) . . ?
C3 C4B C5B 116.2(16) . . ?
N3 C6 C7 109.3(4) . . ?
N4 C7 C6 108.7(3) . . ?
C9 C8 N3 117.3(4) . . ?
C8 C9 C10 111.4(5) . . ?
O4 Cl1 O3 115.1(3) . . ?
O4 Cl1 O2 107.0(2) . . ?
O3 Cl1 O2 108.0(2) . . ?
O4 Cl1 O1 108.5(2) . . ?
O3 Cl1 O1 107.2(2) . . ?
O2 Cl1 O1 111.1(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N4 2.088(3) . ?
Ni1 N2 2.090(3) . ?
Ni1 N5 2.113(3) . ?
Ni1 N3 2.119(3) . ?
Ni1 N7 2.121(3) . ?
Ni1 N1 2.124(4) . ?
N1 C3 1.446(6) . ?
N1 C1 1.505(6) . ?
N2 C2 1.460(6) . ?
N3 C8 1.484(5) . ?
N3 C6 1.485(5) . ?
N4 C7 1.457(5) . ?
N5 N6 1.141(4) . ?
N6 N7 1.126(4) 4_565 ?
N7 N6 1.126(4) 4_566 ?
C1 C2 1.433(7) . ?
C3 C4B 1.246(10) . ?
C3 C4A 1.454(14) . ?
C4A C5A 1.477(18) . ?
C4B C5B 1.531(17) . ?
C6 C7 1.501(6) . ?
C8 C9 1.456(6) . ?
C9 C10 1.526(7) . ?
Cl1 O4 1.401(3) . ?
Cl1 O3 1.404(3) . ?
Cl1 O2 1.405(3) . ?
Cl1 O1 1.423(3) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N4 Ni1 N1 C3 61.9(4) . . . . ?
N2 Ni1 N1 C3 -118.2(4) . . . . ?
N5 Ni1 N1 C3 -32.6(4) . . . . ?
N3 Ni1 N1 C3 173(6) . . . . ?
N7 Ni1 N1 C3 149.3(4) . . . . ?
N4 Ni1 N1 C1 -166.0(3) . . . . ?
N2 Ni1 N1 C1 13.9(3) . . . . ?
N5 Ni1 N1 C1 99.5(3) . . . . ?
N3 Ni1 N1 C1 -55(6) . . . . ?
N7 Ni1 N1 C1 -78.6(3) . . . . ?
N4 Ni1 N2 C2 -174(100) . . . . ?
N5 Ni1 N2 C2 -79.0(3) . . . . ?
N3 Ni1 N2 C2 -168.2(3) . . . . ?
N7 Ni1 N2 C2 96.6(3) . . . . ?
N1 Ni1 N2 C2 12.9(3) . . . . ?
N4 Ni1 N3 C8 115.8(3) . . . . ?
N2 Ni1 N3 C8 -64.2(3) . . . . ?
N5 Ni1 N3 C8 -149.9(3) . . . . ?
N7 Ni1 N3 C8 28.2(3) . . . . ?
N1 Ni1 N3 C8 5(6) . . . . ?
N4 Ni1 N3 C6 -12.8(2) . . . . ?
N2 Ni1 N3 C6 167.3(2) . . . . ?
N5 Ni1 N3 C6 81.6(2) . . . . ?
N7 Ni1 N3 C6 -100.3(3) . . . . ?
N1 Ni1 N3 C6 -124(6) . . . . ?
N2 Ni1 N4 C7 -11(11) . . . . ?
N5 Ni1 N4 C7 -106.0(3) . . . . ?
N3 Ni1 N4 C7 -16.9(2) . . . . ?
N7 Ni1 N4 C7 78.4(3) . . . . ?
N1 Ni1 N4 C7 162.0(3) . . . . ?
N4 Ni1 N5 N6 28.4(5) . . . . ?
N2 Ni1 N5 N6 -151.0(5) . . . . ?
N3 Ni1 N5 N6 -55.1(5) . . . . ?
N7 Ni1 N5 N6 147.3(16) . . . . ?
N1 Ni1 N5 N6 125.4(5) . . . . ?
Ni1 N5 N6 N7 8(70) . . . 4_565 ?
N4 Ni1 N7 N6 -106.9(8) . . . 4_566 ?
N2 Ni1 N7 N6 72.5(8) . . . 4_566 ?
N5 Ni1 N7 N6 133.9(15) . . . 4_566 ?
N3 Ni1 N7 N6 -23.6(8) . . . 4_566 ?
N1 Ni1 N7 N6 156.0(8) . . . 4_566 ?
C3 N1 C1 C2 93.5(6) . . . . ?
Ni1 N1 C1 C2 -40.4(6) . . . . ?
N1 C1 C2 N2 56.1(7) . . . . ?
Ni1 N2 C2 C1 -40.1(5) . . . . ?
C1 N1 C3 C4B 156.5(14) . . . . ?
Ni1 N1 C3 C4B -76.9(14) . . . . ?
C1 N1 C3 C4A 83.2(12) . . . . ?
Ni1 N1 C3 C4A -150.2(10) . . . . ?
C4B C3 C4A C5A 50(2) . . . . ?
N1 C3 C4A C5A 167.4(18) . . . . ?
N1 C3 C4B C5B -162.6(18) . . . . ?
C4A C3 C4B C5B -56(2) . . . . ?
C8 N3 C6 C7 -89.4(4) . . . . ?
Ni1 N3 C6 C7 40.1(4) . . . . ?
Ni1 N4 C7 C6 43.7(4) . . . . ?
N3 C6 C7 N4 -57.9(5) . . . . ?
C6 N3 C8 C9 -74.3(5) . . . . ?
Ni1 N3 C8 C9 161.8(4) . . . . ?
N3 C8 C9 C10 -176.0(4) . . . . ?
